CN108483518A - A kind of preparation method with cross-linked network wall construction NiO materials - Google Patents
A kind of preparation method with cross-linked network wall construction NiO materials Download PDFInfo
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Abstract
A kind of preparation method with cross-linked network wall construction NiO materials, it is related to a kind of preparation method of NiO crosslinkings leader gas sensitive.The present invention is to solve the technical problem that existing NiO nm walls are of high cost, optimum working temperature is high.This method is as follows：Gas sensor substrate is immersed and keeps open magnetic agitation in nickel amine complex aqueous solution at room temperature, waits for NH3After volatilization, gas sensor substrate is taken out, rinses its surface with deionized water, and dry, is sintered, NiO crosslinking leader gas sensors are obtained.The optimum working temperature of material of the present invention is only 50 DEG C, well below most of Metal oxide semiconductor gas-sensitiveness material；It is to 100ppm H2The response sensitivity of S gases reaches 137.26, and minimum detection limit shows splendid H down to 10ppb2S selectivity, the invention belongs to H2The preparation field of S gas sensitives.
Description
Technical field
The present invention relates to a kind of preparation methods with cross-linked network wall construction NiO materials.
Background technology
Hydrogen sulfide be it is a kind of there is corrosivity and flammable toxic gas, when low concentration, can influence the vision system of human body
System, respiratory system and central nervous system, even life-threatening when high concentration.For example, when being exposed to 2ppm H2When S gases, roar
There is bronchoconstriction in asthma patient；When 5ppm, human body feels ophthalmic uncomfortable；When 7-14ppm, blood lactic acid concentration increases, bone
Flesh citrate synthase activity declines, and oxygen uptake declines；When 28ppm, occur tired, lose the appetite, headache is irritated, it is dizzy and
The symptoms such as memory decrease；When its concentration further increases, it is many serious that human body smell paralysis, respiratory distress etc. can be caused
Consequence；If H2S concentration is more than 700ppm, it might even be possible to lead to death.Human health is seriously threatened in view of it, the U.S. cares for
Ask that the H in living environment suggests in the committee2S gases threshold value should be less than 80ppb.Therefore, exploitation is a kind of having highly sensitive, Gao Xuan
Selecting property, it is low detection limit, low energy consumption H2S gas sensors have important actual application value.As classical traditional air-sensitive material
Material, metal-oxide semiconductor (MOS) (such as ZnO, In2O3, NiO, Fe2O3, WO3, SnO2, MoO3Deng) it has been widely used in H2S gases
Sensor field.Wherein, NiO becomes most promising H by its excellent chemical stability and significant electric property2S
One of gas sensitive material.The NiO nanometer wall constructions being especially prepared in situ in substrate, due to having and electrode associativity
It is good, a plurality of air ventilation passage, larger specific surface area and more active site can be provided, and are easy to electron-transport etc.
Advantage and receive much attention.The existing method that NiO nm walls are prepared in situ in substrate is hydrothermal synthesis method, and this method needs make
It is reacted at 200 DEG C with from pressure reaction kettle, instrument cost is high, and preparation condition is harsh, cumbersome, is not easy to industrialize, and
It is difficult to remove containing sulphur impurity in obtained NiO nm walls.In addition, the best work of the NiO nm wall gas sensors finally obtained
It is 92 DEG C to make temperature, and energy consumption is larger, makes troubles for practical application.
Invention content
The purpose of the present invention is to solve existing method prepare NiO nm walls are of high cost, optimum working temperature is high
Technical problem provides a kind of a kind of preparation side with cross-linked network wall construction NiO materials of low cost, low operating temperatures
Method.
Preparation method with cross-linked network wall construction NiO materials follows the steps below：
One, 2.24-5.97g nickel acetates are poured into 300mL deionized waters, makes it completely dissolved, obtains under magnetic agitation
Green Ni-acetate solution；
Two, the ammonium hydroxide that 15-50mL mass concentrations are 25% is added into the solution obtained by step 1, obtains blue solubility
Nickel-amine complex aqueous solution；
Three, immerse substrate in nickel-amine complex aqueous solution keeps magnetic agitation 18-36h room temperatures to volatilize at room temperature
NH3, green Ni (OH) is grown in substrate2Nm wall thin film precursor, substrate is taken out, its surface is rinsed with deionized water, and
It is dried at 60 DEG C；
Four, it will be placed in Muffle furnace by the substrate of step 3 processing, 500-800 DEG C of sintering 2h is obtained with cross-linked network
The H of wall construction2S gas sensitive materials (surface growth has the gas sensor of NiO crosslinking leaders)；
A piece resistive heater is inserted into NiO crosslinking leader gas sensors, and by its integral solder on pedestal,
At 100 DEG C aging for 24 hours, for carrying out H2S gas sensitization performances are tested.
Substrate described in step 3 is to be coated with the alumina ceramic tube, glass substrate or carbon cloth of gold electrode.
The alumina ceramic tube that gold electrode is coated with described in step 3 is that there are two the oxygen of the parallel gold electrode at a distance of 1mm for plating
Change aluminium ceramic tube, ceramics pipe range 4mm, internal diameter 0.8mm, each gold electrode is welded with two platinum filaments.
Room temperature described in step 3 is 25 DEG C.
The present invention provide it is a kind of it is new, inexpensive, easy, be easy to industrialized method, be prepared in situ in substrate
NiO cross-linked network wall construction materials, and H in environment can be applied to2The monitoring of S gases.Utilize appropriate ammonium hydroxide and nickel acetate
Soluble nickel-amine complex aqueous solution is formed, slowly volatilize NH at room temperature3, in-situ deposition Ni (OH) in substrate2Nm wall
Presoma, finally sintering obtains NiO crosslinking leader gas sensors at 500-800 DEG C.
Compared with prior art, the present invention has the advantages that：
(1) there is not been reported for the NiO gas sensitives with cross-linked network wall construction in the present invention.
(2) preparation method in the present invention is extremely simple, and of low cost, mild condition is easy to industrialization large-scale production.
(3) NiO in the present invention is crosslinked leader gas sensitive stable structure, and pattern is uniform, and has excellent H2S gases
Sensitivity characteristic and splendid H2S gas-selectivelies.The optimum working temperature of material of the present invention is only 50 DEG C, well below absolutely mostly
Several Metal oxide semiconductor gas-sensitiveness materials；It is to 100ppm H2The response sensitivity of S gases reaches 137.26, minimum inspection
Limit is surveyed down to 10ppb, is significantly better than most of H2S gas sensors, and sensitivity and H2In good between S gas concentrations
Good linear relationship has huge application value.
(4) using the method in the present invention, NiO crosslinking leaders can not only be prepared in situ on alumina ceramic tube, also
Can be prepared in situ on glass substrate and carbon cloth NiO crosslinking leader film, be NiO films in ultracapacitor, lithium-ion electric
Solid foundation is established in the application in the fields such as pond, electrochemical sensing.
Description of the drawings
Fig. 1 is the electronic photo for testing substrate in a step 3；
Fig. 2 is Ni (OH) in one step 3 of experiment2Nm wall film precursor grows the scanning electron microscope (SEM) photograph of 3h；
Fig. 3 is Ni (OH) in one step 3 of experiment2Nm wall thin film precursor grows the scanning electron microscope (SEM) photograph of 6h；
Fig. 4 is Ni (OH) in one step 3 of experiment2Nm wall thin film precursor grows the scanning electron microscope (SEM) photograph of 9h；
Fig. 5 is Ni (OH) in one step 3 of experiment2Nm wall thin film precursor grows the scanning electron microscope (SEM) photograph of 12h；
Fig. 6 is Ni (OH) in one step 3 of experiment2Nm wall thin film precursor grows the scanning electron microscope (SEM) photograph of 16h；
Fig. 7 is Ni (OH) in one step 3 of experiment2The scanning electron microscope (SEM) photograph of nm wall thin film precursor growth for 24 hours；
Fig. 8 is Ni (OH) in one step 3 of experiment2Nm wall thin film precursor grows the scanning electron microscope of cross section when for 24 hours
Figure；
Fig. 9 is the XRD spectrum for testing precursor powder after 60 DEG C of drying in a step 3；
Figure 10 is Ni (OH) in one step 4 of experiment2Scanning electron microscope of the nm wall thin film precursor after 500 DEG C of sintering 2h
Figure；
Figure 11 is Ni (OH) in one step 4 of experiment2Scanning electron microscope of the nm wall thin film precursor after 600 DEG C of sintering 2h
Figure；
Figure 12 is Ni (OH) in one step 4 of experiment2Scanning electron microscope of the nm wall thin film precursor after 700 DEG C of sintering 2h
Figure；
Figure 13 is Ni (OH) in one step 4 of experiment2Scanning electron microscope of the nm wall thin film precursor after 800 DEG C of sintering 2h
Figure；
Figure 14 is Ni (OH) in one step 4 of experiment2Nm wall thin film precursor is sintered sample powder after 2h at 500-800 DEG C
The XRD spectrum at end；
Figure 15 is to test the NiO obtained after 500-800 DEG C of sintering in one to be crosslinked leader gas sensor in different operating temperature
Under to 50ppm H2The response sensitivity curve of S gases；
Figure 16 is to test the NiO crosslinking leader gas sensors obtained after 700 DEG C of sintering in one when operating temperature is 50 DEG C
To 0.01-0.5ppm H2The response recovery curve of S gases；
Figure 17 is to test the NiO crosslinking leader gas sensors obtained after 700 DEG C of sintering in one when operating temperature is 50 DEG C
To 1-100ppm H2The response recovery curve of S gases；
Figure 18 is to test the NiO crosslinking leader gas sensors obtained after 700 DEG C of sintering in one when operating temperature is 50 DEG C
Response sensitivity and H2Relation curve between S gas concentrations (0.01-0.5ppm)；
Figure 19 is to test the NiO crosslinking leader gas sensors obtained after 700 DEG C of sintering in one when operating temperature is 50 DEG C
Response sensitivity and H2Relation curve between S gas concentrations (1-100ppm)；
Figure 20 is to test the NiO crosslinking leader gas sensors obtained after 700 DEG C of sintering in one when operating temperature is 50 DEG C
It is the response sensitivity block diagram of 8 kinds of gas with various of 50ppm to concentration；
Figure 21 is the scanning electron microscope (SEM) photograph for testing gained NiO crosslinking leader films on glass substrate in two；
Figure 22 is the scanning electron microscope (SEM) photograph for testing gained NiO crosslinking leader films on carbon cloth in two.
Specific implementation mode
Technical solution of the present invention is not limited to act specific implementation mode set forth below, further includes between each specific implementation mode
Arbitrary combination.
Specific implementation mode one：Preparation method with cross-linked network wall construction NiO materials follows the steps below：
One, 2.24-5.97g nickel acetates are poured into the 500ml beakers for containing 300mL deionized waters, is made under magnetic agitation
It is completely dissolved, and obtains green Ni-acetate solution；
Two, the ammonium hydroxide that 15-50mL mass concentrations are 25% is added into the solution obtained by step 1, obtains blue solubility
Nickel-amine complex aqueous solution；
Three, substrate is immersed in nickel-amine complex aqueous solution, keeps opening magnetic agitation -18-36h with slow at room temperature
Slow vaporization NH3, by room temperature volatilization NH3Afterwards, green Ni (OH) is grown in substrate2Nm wall thin film precursor, substrate is taken
Go out, rinses its surface with deionized water, and dried at 60 DEG C；
Four, it will be placed in Muffle furnace by the substrate of step 3 processing, 500-800 DEG C of sintering 2h is obtained with cross-linked network
The H of wall construction2S gas sensitive materials (NiO is crosslinked leader gas sensor)；
A piece resistive heater is inserted into NiO crosslinking leader gas sensors, and by its integral solder on pedestal,
At 100 DEG C aging for 24 hours, for carrying out H2S gas sensitization performances are tested.
Specific implementation mode two：The present embodiment is different from the first embodiment in that the substrate described in step 3 is
It is coated with the alumina ceramic tube, glass substrate or carbon cloth of gold electrode.It is other same as the specific embodiment one.
Specific implementation mode three：Unlike one of present embodiment and specific implementation mode one or two described in step 3
Room temperature be 25 DEG C.It is other identical as one of specific implementation mode one or two.
Specific implementation mode four：It will in step 1 unlike one of present embodiment and specific implementation mode one to three
3.75g nickel acetates pour into 300mL deionized waters, are allowed to be completely dissolved under magnetic agitation, obtain green Ni-acetate solution.It is other
It is identical as one of specific implementation mode one to three.
Specific implementation mode five：To step in step 2 unlike one of present embodiment and specific implementation mode one to four
The ammonium hydroxide that 25mL mass concentrations are 25% is added in the solution of a rapid gained, obtains blue soluble nickel-amine complex aqueous solution.
It is other identical as one of specific implementation mode one to four.
Specific implementation mode six：To step in step 2 unlike one of present embodiment and specific implementation mode one to five
Substrate is immersed in nickel-amine complex aqueous solution in rapid three and keeps magnetic agitation room temperature volatilization for 24 hours NH at room temperature3, in substrate
Grow green Ni (OH)2Nm wall thin film precursor.It is other identical as one of specific implementation mode one to five.
Specific implementation mode seven：Unlike one of present embodiment and specific implementation mode one to six described in step 3
The alumina ceramic tube for being coated with gold electrode is that there are two the alumina ceramic tube of the parallel gold electrode at a distance of 1mm, the ceramic tubes for plating
Long 4mm, internal diameter 0.8mm, each gold electrode are welded with two platinum filaments.It is other identical as one of specific implementation mode one to six.
Using following experimental verifications effect of the present invention：
Experiment one：
A kind of preparation method with cross-linked network wall construction NiO materials：
One, 3.75g nickel acetates are weighed, are poured into the 500mL beakers for containing 300mL deionized waters, under magnetic agitation
It is allowed to be completely dissolved, obtains the Ni-acetate solution of a concentration of 0.05mol/L of green.
Two, under magnetic agitation, the ammonium hydroxide that 25mL mass concentrations are 25% is added dropwise into Ni-acetate solution, obtaining blue can
Dissolubility nickel-amine complex aqueous solution.
Three, substrate (alumina ceramic tube for being coated with gold electrode) is immersed in nickel-amine complex aqueous solution, in 25 DEG C of holdings
Open magnetic agitation is for 24 hours with the NH that slowly volatilizees3, by room temperature volatilization NH3Afterwards, green Ni (OH) is grown in substrate2Nm wall is thin
Film precursor takes out substrate, rinses its surface with deionized water, and dried at 60 DEG C.
Four, surface growth there is into Ni (OH)2The substrate of nm wall thin film precursor is placed in Muffle furnace, at 500-800 DEG C
It is sintered 2h, obtains with cross-linked network wall construction NiO materials (NiO is crosslinked leader gas sensor)；
A piece resistive heater, which is inserted into, to be had in cross-linked network wall construction NiO materials (NiO is crosslinked leader gas sensor), and
By its integral solder on pedestal, at 100 DEG C aging for 24 hours, for carrying out H2S gas sensitization performances are tested.
Air-sensitive performance is tested：The air-sensitive performance that NiO is crosslinked leader gas sensor is measured using static distribution test method.In advance
It will first be vacuumized in 10L hermetical testings cabin with pump, be then injected into the object gas of certain volume, then with fresh air balance test
Pressure inside and outside cabin, to obtain the test gas of respective concentration, calculation formula：Gas concentration (ppm)=injection gas volume ×
106/ test warehouse product.The operating temperature of gas sensor is controlled by adjusting the voltage being applied on resistive heater.
The gas of gas sensor responds and recovery characteristics, is inserted and removed from the resistance variations of test chamber by it to characterize.Gas response spirit
Sensitivity (S) is defined as：S=Rg/Ra, wherein RaIndicate resistance value of the gas sensor in pure air, RgIndicate gas sensor
The resistance value in gas is tested in a certain concentration.
Fig. 1 is the electronic photo of substrate, which is that there are two the aluminium oxide ceramics of parallel gold electrode (at a distance of 1mm) for plating
Pipe, long 4mm, internal diameter 0.8mm, outer diameter 1.2mm, hollow space are inserted into resistive heater, change heating voltage to provide not
Same operating temperature, each gold electrode are welded with two platinum filaments, for being connect with air-sensitive test system.
Fig. 2-Fig. 7 can see Ni (OH)2Nm wall presoma is in the growth course on gas sensor surface, Ni (OH)2Forerunner
Body is deposited on substrate surface in the form of nano-particle first, starts vertical-growth Ni (OH) after being covered with substrate surface2Nanometer
Piece forms the nanometer wall construction being cross-linked with each other after deposition for 24 hours.
It can be seen that presoma Ni (OH) in Fig. 82It is regularly grown on substrate surface, the height of nm wall is about 260nm
Left and right.
Fig. 9 is the XRD spectrum of precursor powder after 60 DEG C of drying, the X-ray diffraction peak position of precursor powder and Ni
(OH)2JCPDS cards (14-0117) are completely the same, illustrate that the object of presoma is mutually Ni (OH)2。
It can see in Figure 10-Figure 13, Ni (OH)2Nm wall presoma starts after 500 DEG C of sintering on nm wall
Existing pore structure forms NiO and is crosslinked leader；After 600 DEG C of sintering, pore structure becomes larger；After 700 DEG C of sintering, pore structure further increases；
After 800 DEG C of sintering, together, pore structure becomes smaller adjacent particle for bond vitrified at high temperature.
Figure 14 is Ni (OH)2XRD spectrum of the nm wall precursor powder after 500-800 DEG C of sintering 2h, as seen from the figure, sample
The X-ray diffraction peak position of product powder is completely the same with NiO JCPDS cards (47-1049), illustrates that sample passes through 500-800
DEG C sintering after can be by Ni (OH)2Dehydration is changed into NiO object phases, and increases with the diffraction peak intensity for increasing sample of sintering temperature
By force, crystallization degree increases.
It is in Figure 15 it can be seen that aobvious when operating temperature is 50 DEG C through 700 DEG C of sintered NiO crosslinking leader gas sensors
Highest response sensitivity is shown, it is to 50ppm H at 50 DEG C2The response sensitivity of S can reach 67.01.
It can be seen that being in operating temperature through 700 DEG C of sintered NiO crosslinkings leader gas sensors from Figure 16 and Figure 17
At 50 DEG C, to H in 0.01-100ppm concentration ranges2S gases generate significant resistance variations, to 100ppm H2The spirit of S gases
Sensitivity is up to 137.26, and minimum detection limit can be completely recovered to it down to 0.01ppm (10ppb) in recovery process
Initial resistance value shows excellent H2S gas sensitization performances.
Response sensitivity and H when Figure 18 and Figure 19 is 50 DEG C2Relation curve between S gas concentrations, responds as seen from the figure
Sensitivity is respectively within the scope of 0.01-1ppm and 1-100ppm and H2It is in good linear relationship, fitting system between S gas concentrations
Number R2Respectively 0.9955 (0.01-1ppm) and 0.9969 (1-100ppm), this characteristic are that the gas sensitive is real in the environment
When monitor H2S gases are laid a good foundation.
It can be seen that the NiO crosslinking leader gas sensors obtained after 700 DEG C of sintering are when operating temperature is 50 DEG C in Figure 20
To 50ppm H2The sensitivity of S reaches 67.01, and to concentration be all the ammonia of 50ppm, ethyl alcohol, formaldehyde, acetone, aniline, benzene,
The response sensitivity of trimethylamine is respectively less than 2, shows to H2The splendid selectivity of S gases.
Experiment two：
A kind of preparation method with cross-linked network wall construction NiO materials：
One, 3.75g nickel acetates are weighed, are poured into the 500mL beakers for containing 300mL deionized waters, under magnetic agitation
It is allowed to be completely dissolved, obtains the Ni-acetate solution of a concentration of 0.05mol/L of green.
Two, under magnetic agitation, the ammonium hydroxide that 25mL mass concentrations are 25% is added dropwise into Ni-acetate solution, obtaining blue can
Dissolubility nickel-amine complex aqueous solution.
Three, glass substrate is immersed in nickel-amine complex aqueous solution, keeps open magnetic agitation for 24 hours with slow in 25 DEG C
Volatilize NH3, by room temperature volatilization NH3Afterwards, green Ni (OH) is grown in substrate2Nm wall thin film precursor, substrate is taken out,
Its surface is rinsed with deionized water, and is dried at 60 DEG C.
Four, surface growth there is into green Ni (OH)2The substrate of nm wall film is placed in Muffle furnace, and 2h is sintered at 500 DEG C,
It obtains with cross-linked network wall construction NiO materials.
Experiment three：
A kind of preparation method with cross-linked network wall construction NiO materials：
One, 3.75g nickel acetates are weighed, are poured into the 500mL beakers for containing 300mL deionized waters, under magnetic agitation
It is allowed to be completely dissolved, obtains the Ni-acetate solution of a concentration of 0.05mol/L of green.
Two, under magnetic agitation, the ammonium hydroxide that 25mL mass concentrations are 25% is added dropwise into Ni-acetate solution, obtaining blue can
Dissolubility nickel-amine complex aqueous solution.
Three, carbon cloth is immersed in nickel-amine complex aqueous solution, keeps open magnetic agitation for 24 hours slowly to volatilize in 25 DEG C
NH3, by room temperature volatilization NH3Afterwards, green Ni (OH) is grown in substrate2Nm wall thin film precursor, substrate is taken out, and spends
Ionized water rinses its surface, and is dried at 60 DEG C.
Four, surface growth there is into green Ni (OH)2The substrate of nm wall film is placed in Muffle furnace, and 2h is sintered at 500 DEG C,
It obtains with cross-linked network wall construction NiO materials.
It can be seen that, it can be succeeded using the method for the present invention and be had on glass substrate and carbon cloth in Figure 21 and Figure 22
The NiO films of crosslinking leader structure are NiO porous films in necks such as ultracapacitor, lithium ion battery, electrochemical sensings
Solid foundation is established in the application in domain.
Claims (7)
1. a kind of preparation method with cross-linked network wall construction NiO materials, it is characterised in that one kind having cross-linked network wall construction NiO
The preparation method of material follows the steps below：
One, 2.24-5.97g nickel acetates are poured into 300mL deionized waters, is made it completely dissolved under magnetic agitation, obtains green
Ni-acetate solution；
Two, the ammonium hydroxide that 15-50mL mass concentrations are 25% is added into the solution obtained by step 1, obtains blue soluble nickel-
Amine complex aqueous solution；
Three, substrate is immersed in nickel-amine complex aqueous solution and keeps magnetic agitation 18-36h room temperatures volatilization NH at room temperature3, substrate
On grow green Ni (OH)2Nm wall thin film precursor, substrate is taken out, and rinses its surface with deionized water, and in 60 DEG C
Lower drying；
Four, it will be placed in Muffle furnace by the substrate of step 3 processing, 500-800 DEG C of sintering 2h is obtained a kind of with cross-linked network
The NiO materials of wall construction.
2. a kind of preparation method with cross-linked network wall construction NiO materials according to claim 1, it is characterised in that step 1
It is middle to pour into 3.75g nickel acetates in 300mL deionized waters, it is allowed to be completely dissolved under magnetic agitation, obtains green Ni-acetate solution.
3. a kind of preparation method with cross-linked network wall construction NiO materials according to claim 1, it is characterised in that step 2
The ammonium hydroxide that 25mL mass concentrations are 25% is added in the middle solution to obtained by step 1, obtains blue soluble nickel-amine complex
Aqueous solution.
4. a kind of preparation method with cross-linked network wall construction NiO materials according to claim 1, it is characterised in that step 2
Middle immerse substrate in nickel-amine complex aqueous solution into step 3 keeps magnetic agitation room temperature volatilization for 24 hours NH at room temperature3,
Green Ni (OH) is grown in substrate2Nm wall thin film precursor.
5. a kind of preparation method with cross-linked network wall construction NiO materials according to claim 1, it is characterised in that step 3
Described in substrate be to be coated with the alumina ceramic tube, glass substrate or carbon cloth of gold electrode.
6. a kind of preparation method with cross-linked network wall construction NiO materials according to claim 1, it is characterised in that step 3
Described in room temperature be 25 DEG C.
7. a kind of preparation method with cross-linked network wall construction NiO materials according to claim 1, it is characterised in that step 3
Described in be coated with gold electrode alumina ceramic tube be plating there are two at a distance of 1mm parallel gold electrode alumina ceramic tube, should
Ceramic pipe range 4mm, internal diameter 0.8mm, each gold electrode are welded with two platinum filaments.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1107442A (en) * | 1994-02-26 | 1995-08-30 | 王维波 | Process for preparing nickel hydroxide |
| CN102887551A (en) * | 2012-10-12 | 2013-01-23 | 金川集团股份有限公司 | Porous spherical nickel protoxide and preparation method thereof |
| CN103043731A (en) * | 2013-02-04 | 2013-04-17 | 苏州纳格光电科技有限公司 | Preparation method of nickel oxide nanosheet and formaldehyde sensor |
| CN106944065A (en) * | 2017-03-27 | 2017-07-14 | 江苏金聚合金材料有限公司 | The preparation method and application of graphene-supported nickel hydrogenation catalyst |
-
2018
- 2018-01-31 CN CN201810097809.9A patent/CN108483518B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1107442A (en) * | 1994-02-26 | 1995-08-30 | 王维波 | Process for preparing nickel hydroxide |
| CN102887551A (en) * | 2012-10-12 | 2013-01-23 | 金川集团股份有限公司 | Porous spherical nickel protoxide and preparation method thereof |
| CN103043731A (en) * | 2013-02-04 | 2013-04-17 | 苏州纳格光电科技有限公司 | Preparation method of nickel oxide nanosheet and formaldehyde sensor |
| CN106944065A (en) * | 2017-03-27 | 2017-07-14 | 江苏金聚合金材料有限公司 | The preparation method and application of graphene-supported nickel hydrogenation catalyst |
Non-Patent Citations (1)
| Title |
|---|
| GUANGHUI LI ET AL.: "Controllable Synthesis of 3D Ni(OH)2 and NiO Nanowalls on Various Substrates for High-Performance Nanosensors", 《SMALL》 * |
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